A new method combining QuEChERS (quick, easy, cheap, effective, rugged and safe) and DLLME (dispersive liquid–liquid microextraction) for the simultaneous determination of residues of ten sulfonylurea herbicide in wa...A new method combining QuEChERS (quick, easy, cheap, effective, rugged and safe) and DLLME (dispersive liquid–liquid microextraction) for the simultaneous determination of residues of ten sulfonylurea herbicide in water using UPLC-MS/MS was developed and validated. Analytes were extracted and purified with QuEChERS and concentrated in chlorobenzene by applying the DLLME procedure. Several extraction parameters were tested, such as volume, extractive solvent by the QuEChERS method and subsequently used for DLLME, selection of extractive solvent and its volume, was tested. The developed method was validated on the basis of international guidelines. Mean recoveries ranged from 81.2 to 104.9%. Repeatability and reproducibility were lower than 10%. Limits of detection (LODs) and quantification (LOQs) were below 0.074 μg/L and 0.244 μg/L, respectively. Decision limit (CCα) and detection capability (CCβ) were calculated and CCβ ranged from 0.101 μg/L (pyrazosulfuron-ethyl) to 0.260 μg/L (nicosulfuron). Finally, when the method was applied to real samples, traces of three compounds were found in 42 samples and only thifensulfuon-methyl was detected above the LOQ in three samples at 0.17-0.20 μg/L.展开更多
文摘A new method combining QuEChERS (quick, easy, cheap, effective, rugged and safe) and DLLME (dispersive liquid–liquid microextraction) for the simultaneous determination of residues of ten sulfonylurea herbicide in water using UPLC-MS/MS was developed and validated. Analytes were extracted and purified with QuEChERS and concentrated in chlorobenzene by applying the DLLME procedure. Several extraction parameters were tested, such as volume, extractive solvent by the QuEChERS method and subsequently used for DLLME, selection of extractive solvent and its volume, was tested. The developed method was validated on the basis of international guidelines. Mean recoveries ranged from 81.2 to 104.9%. Repeatability and reproducibility were lower than 10%. Limits of detection (LODs) and quantification (LOQs) were below 0.074 μg/L and 0.244 μg/L, respectively. Decision limit (CCα) and detection capability (CCβ) were calculated and CCβ ranged from 0.101 μg/L (pyrazosulfuron-ethyl) to 0.260 μg/L (nicosulfuron). Finally, when the method was applied to real samples, traces of three compounds were found in 42 samples and only thifensulfuon-methyl was detected above the LOQ in three samples at 0.17-0.20 μg/L.
